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Analytical Chemistry Theoretical and Metrological Fundamentals K Analytical Chemistry Theoretical and Metrological Fundamentals K. Danzer Analytical Chemistry Theoretical and Metrological Fundamentals With 138 Figures and 31 Tables K. Danzer Am Friedensberg 4 07745 Jena Germany e-mail: [email protected] Library of Congress Control Number 2006932265 ISBN-10 3-540-35988-5 Springer Berlin Heidelberg New York ISBN-13 978-3-540-35988-3 Springer Berlin Heidelberg New York DOI 10.1007/b103950 This work is subject to copyright. All rights are reserved, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilm or in other ways, and storage in data banks. Duplication of this publication or parts thereof is permitted only under the provisions of the German Copyright Law of September 9, 1965, in its current version, and permission for use must always be obtained from Springer. Violations are liable to prosecution under German Copyright Law. Springer is a part of Springer Science+Business Media springer.com © Springer-Verlag Berlin Heidelberg 2007 The use of general descriptive names, registered names, trademarks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. Product liability:The publishers cannot guarantee the accuracy of any information about dosage and appli- cation contained in this book. In every individual case the user must check such information by consulting the relevant literature. Cover-Design: WMXDesign GmbH, Heidelberg Typesetting: PTP-Berlin Protago-TEX-Production GmbH, Germany Production: LE-TEX Jelonek, Schmidt & V¨ockler GbR, Leipzig, Germany Printed on acid-free paper 2/3141/YL-543210 Preface Analytical chemistry can look back on a long history. In the course of its de- velopment, analytical chemistry has contributed essentially to the progress of diverse ˇelds of science and technology. Signiˇcant progress in natu- ral philosophy, chemistry and other disciplines has been founded on re- sults and discoveries in analytical chemistry. Well known examples include Archimedes' principle, iatrochemistry, emergence and overcoming of phlo- giston theory, basic chemical laws on stoichiometry and mass proportions as well as the discoveries of elements and of nuclear ˇssion. As chemistry split into inorganic, organic and physical chemistry in the middle of the nineteenth century, the question occasionally arose as to whether analytical chemistry was likewise an autonomous ˇeld of chemistry. At the beginning of the twentieth century, analytical chemistry was estab- lished by Wilhelm Ostwald and other protagonists on the basis of chemical and physicochemical laws and principles. In addition, analytical procedures and instruments spread into other chemical ˇelds. However, in the 1950s and 1960s a new generation of analysts opened their mind to ideas coming from other scientiˇc ˇelds dealing with measurements from other points of view such as information science, metrology, technometrics, etc. As a result, efforts made towards the acceptance of analytical chem- istry as an autonomous ˇeld of chemistry increased. Analysts in USA and Europe founded organisations and forums that focussed ideas and devel- opments in progressive directions. In this way, not only were national and international societies formed but also regular conferences like Pittcon and Euroanalysis. In this connection the so-called Lindau circle should be men- tioned where analysts from Germany, Austria and Switzerland made public relevant fundamentals of analytical chemistry derived from statistics, infor- mation theory, system theory, signal theory, game theory, decision theory, metrology, etc. In parallel with this, such modern principles have been suc- cessfully applied in selected case studies, mainly by scientists from USA, UK, and Canada. From this development, real theoretical and metrolog- ical fundamentals of analytical chemistry have crystallized. However, the acceptance of analytical chemistry as an automomous branch of chemistry has not been realised. Gradually, however, progress in analytical chemistry culminated in the 1990s in the proclamation of a new scientiˇc discipline, analytical science. Protagonists of these activities included Michael Widmer and Klaus Doerffel. VI Preface Today, analytical chemistry is still a discipline within chemistry. Al- though characterized as an auxiliary science, analytical chemistry continues to develop and grow just as before. It is no detraction being characterized as an auxiliary discipline as mathematics shows. However, it is likely that efforts to make analytical chemistry a more independent science will be repeated in the future from time to time. Analytical chemistry possesses today a sound basis of chemical, physical, methodical, metrological, and theoretical fundamentals. The ˇrst of these are usually taken as the basis of classical textbooks on analytical chemistry. The others are found in diverse publications in the ˇeld of analytical chem- istry and chemometrics. It is essential to state that chemometrics is not the theoretical basis of analytical chemistry but it contributes signiˇcantly to it. Frequently, analytical chemistry is considered to be a measuring science in chemistry. Therefore, its object is the generation, evaluation, interpreta- tion, and validation of measuring signals as well as the characterization of their uncertainty. With this aim, the analyst needs knowledge of the general analytical process, statistics, optimization, calibration, chemometrical data analysis, and performance characteristics. In this book the attempt is made to summarize all the components that can be considered as building blocks of a theory of analytical chemistry. The \building" constructed in this way is a provisional one. It is incomplete and, therefore, extension, reconstruction and rebuilding have to be expected in the future. A large number of mathematical formulas will be found in the book. This may be regarded as a disadvantage particularly because some of them are not readily to apply in daily analytical practice. However, great scientists, explicitly Emanuel Kant, said that a scientiˇc branch contains only so much of science as it applies mathematics. Consequently, all the relationships which can be described mathematically should be so described. It is true despite Werner Heisenbergs statement: Although natural processes can be described by means of simple laws which can be precisely formulated, these laws, on the other hand, cannot directly be applied to actions in practice. Wherever possible, ofˇcial deˇnitions of IUPAC, ISO and other inter- national organizations have been used, in particular in the \Glossary of Analytical Terms" compiled at the end of the book. However, uniformity could not be achieved in every case. In a few instances, special comments and proposals (characterized as such) have been added. Although progress in the ˇeld of harmonization of nomenclature and deˇnitions has been con- siderable, some things still remain to be done. Some of the contents of various sections have been published previously and are, of course quoted verbatim. In this connection the author is grateful to Klaus Doerffel, Karel Eckschlager, Gunter Ehrlich, Andrzej Parczewski, Karol Florian, Mikulas Matherny, Gunter Marx, Dieter Molch, Eberhard Than, Ludwig Kuchler and others for long-standing collaboration resulting in mutually complementary papers and books. A chapter on statistics was previously published in another book (Accreditation and Quality Assurance Preface VII in Analytical Chemistry edited by Helmut Gunzler at Springer). Gratefully I have adapted essential parts of the translation of Gaida Lapitajs here in this book. Stimulations and ideas have arisen from discussions with William Hor- witz, Duncan Thorburn Burns, Alan Townshend, Koos van Staden, and other members of diverse IUPAC Commissions and Task Groups as well as ofˇ- cers of the Analytical Chemistry Division. From a 20-year membership of various IUPAC bodies I have gained a variety of feedback and experience which has proved to be useful in the writing of this book. In particular, I owe Lloyd Currie and Mattias Otto a great debt of gratitude. They have permitted me to use essential parts of common publications on calibration quoted in Chap. 6. Many of the results stem from work carried out with colleagues, collaborators, postdocs and graduate students. All of them are deserving of my thanks but, due to the large numbers involved, this cannot be done here. Some representative colleagues include Jurgen Einax, Hart- mut Hobert, Werner Schron, Manfred Reichenbacher, Reiner Singer, Diet- rich Wienke, Christoph Fischbacher, Kai-Uwe Jagemann, Michael Wagner, Katrin Venth, Raimund Horn, Gabriela Thiel, Demetrio de la Calle GarcÃa, and Balint Berente. The author gratefully acknowledges the cooperation with and the support of the editorial staff of Springer. Particularly I have to thank Peter Enders, Birgit Kollmar-Thoni, and { last but not least { John Kirby, the English copy editor, who has essentially improved the English. Many thanks for that. No book is free of errors and this one will be no exception. Therefore, the author would be grateful to readers who point out errors and mistakes and suggest any improvement. Jena, July 2006 Klaus Danzer Contents Symbols ........................................................ XIII Abbreviations
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